Agenda Item 8 CX/MAS 04/9

JOINT FAO/WHO FOOD STANDARDS PROGRAMME

CODEX COMMITTEE ON METHODS OF ANALYSIS AND SAMPLING

Twenty-fifth Session
Budapest, Hungary, 8 12 March 2004

ENDORSEMENT OF METHODS OF ANALYSIS PROVISIONS IN CODEX STANDARDS

This document contains the Methods of analysis proposed by the following Committees in Draft
Standards and Proposed Draft Standards under elaboration or as a revision of the methods included in
adopted standards.

Part I Methods of Analysis

A. Codex Committee on Fats and Oils
B. Codex Committee on Fish and Fishery Products
C. Ad hoc Intergovernmental Task Force on Fruit and Vegetable Juices
Part II Sampling
Codex Committee on Fats and Oils

Note: Document CX/MAS 04/9-Add.1 on the updating of the methods for additives and contaminants
will be presented separately.
 A. CODEX COMMITTEE ON FATS AND OILS1
1. Draft Standard for Fat Spreads and Blended Spreads (at Step 6)2

COMMODITY PROVISION METHOD PRINCIPLE Note

Fat Spreads and Blended Milk fat content AOAC 985.16 AAS see below
Spreads (butyric acid) CCFO
discussion
IUPAC 2.310, AOAC 990.27 or AOCS Ca Gravimetry
5c-87 (97).

The Committee considered the question from the Codex Committee on Methods of Analysis and Sampling concerning the determination of milk fat. As proposed by the
Working Group on Methods of Analysis and Sampling (CRD 10), the Committee noted that butyric acid was an indicator but that the concentration was subject to
variation. It therefore recommended, in the absence of a single agreed factor, to convert the butyric acid concentration into milk fat concentration, and to report the range
in which the milk fat concentration of a sample would lie. It was also agreed that the method would read Milk Fat Content (butyric acid) for clarification purposes. The
Committee agreed to retain the methods of analysis for salt content and for vitamins at this stage, as these ingredients were mentioned in the standard. However, it noted
that there were no specific levels for these substances and that this question might require further consideration (ALINORM 03/17, para. 60).
2. Standard for Olive Oils and Olive Pomace Oils3

COMMODITY PROVISION METHOD PRINCIPLE Note

Olive Oils and Organoleptic characteristics COI/T.20/Doc. no. 15.
Olive Pomace Oils
Free acidity ISO 660 or AOCS Cd 3d-63(99). Titrimetry
Fatty acid composition COI/T.20/Doc. no. 24 and ISO 5508 Gas chromatography of methyl esters
or AOCS Ch 2-91(02) or AOCS Ce
1f-96 (02)
Trans fatty acids content COI/T.20/Doc no. 17 or ISO Gas chromatography
15304:2001 or AOCS Ce 1f-96 (02)
Wax content COI/T.20/Doc. no. 18 or AOCS Ch 8- Titrimetry
02 (02)
Difference between the actual and COI/T.20/Doc. no. 20 or AOCS Ce 5b- Calculation
theoretical ECN 42 triglyceride 89 (97).
content

1
ALINORM 03/17, Appendices II, III and IV
2
The other methods will be presented to the next session of the CCMAS (April 2005) following the next session of the CCFO (February 2005)
3
The Standard was adopted by the 26th Session of the Commission. The methods had not been endorsed due to the timing of the sessions of CCFO and CCMAS
Olive Oils and Sterol composition and content COI/T.20/Doc. no. 10 or ISO Gas chromatography
Olive Pomace Oils 12228:1999 or AOCS Ch 6-91 (97).
Erythrodiol content IUPAC 2.431. Gas chromatography
Stigmastadienes COl/T.20/Doc. no. 11 or ISO 15788- Gas chromatography
1:1999 or AOCS Cd 26-96 (02).
Peroxide value ISO 3960:2001 or AOCS Cd 8b-90 Titrimetry
(02).
Absorbency in ultra-violet COI/T.20/Doc. no. 19 or ISO Absorption in ultra violet
3656:2001 or AOCS Ch 5-91 (01).
Alpha-tocopherol ISO 9936:1997 HPLC
Arsenic AOAC 952.13 Colorimetry (diethyldithiocarbamate) Type II method for
fats and oils
Arsenic AOAC 942.17 Colorimetry (Molybdenum blue) Type III methods
for fats and oils
Arsenic AOAC 985.16 Colorimetry
Lead AOAC 994.02 or ISO 12193:1994 or AAS Type II method for
AOCS Ca 18c-91(97) fats and oils
Traces of halogenated solvents COI/T.20/Doc. no. 8.
Moisture and volatile matter ISO 662:1998. Gravimetry
Insoluble impurities in light ISO 663:2000. Gravimetry
petroleum
Iron and copper ISO 8294:1994 or AOAC 990.05. Atomic absorption (direct graphite Type II method for
furnace) fats and oils
Saponification value ISO 3657:2002 or AOCS Cd 3-25 (02) Titrimetry
Unsaponifiable matter ISO 3596:2000 or ISO 18609:2000 or Titrimetry Type I method for
AOCS Ca 6b-53 (01) fats and oils
Fatty acids in the 2-position of ISO 6800:1997 or AOCS Ch 3-91 Gas chromatography
the triglycerides (97).
Relative density IUPAC 2.101, with the appropriate Pyknometry
conversion factor.
Refractive index ISO 6320:2000 or AOCS Cc 7-25 (02) Refractometry Type II method for
fats and oils
Iodine value ISO 3961:1996 or AOAC 993.20 or Wijs-Titrimetry Type I method for
AOCS Cd 1d-92 (97) fats and oils

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3. Standard for Named Vegetable Oils4
Amendments proposed to the methods in the current standard for Named Vegetable Oils

COMMODITY PROVISION METHOD PRESENTLY SUGGESTED REPLACEMENT PRINCIPLE NOTE

GIVEN IN STANDARD Current
Type
Named Acidity IUPAC 2.201; or ISO 660: 1996; ISO 660: 1996; or AOCS Cd 3d-63 (99) Titrimetry I
Vegetable Oils or AOCS Cd 3d-63

Apparent density ISO 6883: 2000, with the ISO 6883: 2000, with the appropriate Pyknometry I
appropriate conversion factor; or conversion factor; or AOCS Cc 10c-95 (02)
AOCS Cc 10c-95
Arsenic AOAC 952.13 or IUPAC 3.136 AOAC 952.13 Colorimetry II
(diethyldithiocarbamat
e)
Arsenic AOAC 942.17 AOAC 942.17 or AOAC 985.16 Colorimetry III
(molybdenum blue)
Copper and iron ISO 8294: 1994; IUPAC 2.631; ISO 8294: 1994; or AOAC 990.05; or AOCS AAS (direct graphite II
AOAC 990.05; or AOCS Ca 18b- Ca 18b-91 (97) furnace)
91
Crismer value AOCS Cb 4-35 (97) AOCS Cb 4-35 (97) and AOCS Ca 5a-40 (97) Turbidity I
GLC ranges of Fatty IUPAC 2.301, 2.302 and 2.304; or ISO 5508: 1990 and ISO 5509: 2000; or Gas chromatography II
acid composition ISO 5508: 1990 and ISO 5509: AOCS Ce 2-66 (97); or Ce 1e-91 (01); or Ce of methyl esters
2000; or AOCS Ce 2-66, Ce 1e- 1f-96 (02)
91 or Ce 1f-96
Insoluble impurities IUPAC 2.604; or ISO 663: 2000 ISO 663: 1998 Gravimetry I

4
A Draft Amendment to the Standard was adopted by the 26th Session of the Commission. The amendments to the methods were not endorsed due to the timing of the sessions of
CCFO and CCMAS

4
Named Iodine value (IV) Wijs - IUPAC 2.205/1; ISO 3961: Wijs - ISO 3961: 1996; or AOAC 993.20; or Wijs-Titrimetry I
Vegetable Oils 1996; AOAC 993.20; or AOCS Cd AOCS Cd 1d-1992 (97); or by calculation
1d-1992 (97); or by calculation - AOCS Cd 1b-87 (97) -The method to be used
AOCS Cd 1b-87 (97) for specific named vegetable oils is stipulated
in the Standard
Lead IUPAC 2.632; AOAC 994.02 ; ISO AOAC 994.02 ; or ISO 12193: 1994; or AOCS Atomic Absorption II
12193: 1994; or AOCS Ca 18c-91 Ca 18c-91 (97) (direct graphite
furnace)
Moisture & volatile IUPAC 2.601; or ISO 662: 1998 ISO 662: 1998 Gravimetry (open I
matter at 105C drying)
Peroxide value (PV) IUPAC 2.501 (as amended); or AOCS Cd 8b-90 (02); or ISO 3961: 2001 Titrimetry using iso- I
AOCS Cd 8b 90 (97); or ISO octane
3961: 1998
Refractive index IUPAC 2.102; ISO 6320: 2000; or ISO 6320: 2000; or AOCS Cc 7-25 (02) Refractometry II
AOCS Cc 7-25

Reichert value and IUPAC 2.204 AOCS Cd 5-40 (97) Titrimetry I

Polenske value

Saponification value IUPAC 2.202 or ISO 3657: 1988 ISO 3657: 2002; or AOCS Cd 3-25 (02) Titrimetry I
(SV)

Slip point ISO 6321: 1991 and Amendment 1: ISO 6321:2002 for all oils; or AOCS Cc 3b-92
Open ended capillary I
1998 for all oils; or AOCS Cc 3b- (02); or AOCS Cc 3-25 (97) for Palm Oils only
tube
92; or AOCS Cc 3-25 (97) for Palm
Oils only.
Soap content BS 684 Section 2.5 BS 684 Section 2.5; or AOCS Cc 17-95 (97) Gravimetry I
Sterol content ISO 12228:1999; or IUPAC 2.403 ISO 12228: 1999; or AOCS Ch 6-91 (97) Gas chromatography II
Tocopherol content IUPAC 2.432; or ISO 9936: 1997; ISO 9936: 1997; or AOCS Ce 8-89 (97)
or AOCS Ce 8-89
Unsaponifiable IUPAC 2.401 (part 1-5); or ISO ISO 3596: 2000; or ISO 18609: 2000; or Titrimetry I
matter 3596:2000; or ISO 18609: 2000 AOCS Ca 6b-53 (01)

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 B. CODEX COMMITTEE ON FISH AND FISHERY PRODUCTS5

Draft Standard for Salted Atlantic Herring and Salted Sprats (at Step 8)
Draft Amendment to the Standard for Quick Frozen Fish Sticks (Fish Fingers), Fish Portions and Fish Fillets Breaded or in Batter (at Step 7)

COMMODITY PROVISION METHOD PRINCIPLE

Salted Atlantic Herring and Salted Water content AOAC 950.46B air drying
Sprat
Quick Frozen Fish Sticks Fish content AOAC 966.15 and calculation (see below) see below
(declaration)

Section 7. Sampling, Examination and Analysis

7.4 Estimation of Fish Content
According to AOAC Method 966.15. In cases where there is some remaining doubts over the composition of the fish core then the method of analysis as outlined below
could be used, i.e. as a reference method.
Determination of Fish Content
The fish content of a fish finger (fish stick) is calculated by using the following equation

Weight of ingoing fish

%Fish Content = x100
Weight of final product
For most products therefore, the fish ingredient weight is that of the raw ingredient. Any figure placed or declared on a product label would be a typical quantity
reflecting the producers normal manufacturing variations, in accordance with good manufacturing practice.
Checking of fish content by chemical analysis
The percentage fish content, corrected for the non-fish flesh nitrogen contributed by the carbohydrate coating, is calculated as follows.

(% total nitrogen - % non - fish flesh nitrogen

%Fish = x100
N factor *
* appropriate N (nitrogen) factor
The non-fish flesh nitrogen is calculated as follows: % non-fish flesh nitrogen = % carbohydrate x 0.02

5
ALINORM 04/27/18, Appendix II and Appendix VII (Draft Amendment to the Standard for Quick Frozen Fish Sticks (Fish Fingers), Fish Portions and Fish Fillets Breaded or in
Batter : declaration of fish content)

6
 Where the carbohydrate is calculated by difference: % carbohydrate = 100 (% water + % fat + % protein + % ash)
References
Determination of nitrogen: ISO 937:1978
Determination of moisture: ISO 1442:1997
Determination of total fat: ISO 1443:1973
Determination of ash: ISO 936: 1978

Table 2: Interim Nitrogen factors to be used for white fish as an ingredient (i.e. after GMP)

Nitrogen
SPECIES
%
White fish:
Cod 2.66
Minced Cod 2.61
Coley/Saithe 2.69
European 2.64
Hake
Haddock 2.72
Ling 2.78
Plaice 2.46
Alaskan 2.59
Pollack
Whiting 2.68

2.65
White fish
mean

Additional species important for international trade proposed by Canada, South Africa and the USA but for which there are no nitrogen factors at present:
Pacific Salmon, Atlantic Salmon, Halibut, Sole, Pacific Cod, Pacific Tomcod, Pacific Whiting, Yellowfin Sole and American Catfish
South Africa Hake (Merluccius capensis and Merluccius paradoxus)

C. AD HOC INTERGOVERNMENTAL TASK FORCE ON FRUIT AND VEGETABLE JUICES6

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ALINORM 03/39A, Appendices II and III
7
 Proposed Draft General Standard for Fruit Juices and Nectars 7
The methods listed below were forwarded to the CCMAS by the Task Force on Fruit and Vegetable Juices. However, several methods do not correspond to provisions
in the standard. The list below is presented in conformity with the usual format for endorsement of methods of analysis and identifies those provisions that are included
in the standard, mainly for permitted ingredients and additives and those that are not specified. The report of the Task Force is available on the Codex website at the
following address [Link] and will be available at the CCMAS session for information.
.
COMMODITY PROVISION METHOD PRINCPLE
Fruit Juices and Not specified Determination of Acetic acid Enzymatic determination
Nectars EN 12632 or IFU Method No 66 (1996)
Not specified Determination of Alcohol (ethanol) Enzymatic determination
IFU Method No 52 (1983/1996)
Not specified Determination of anthocyanins HPLC
IFU Method No 71 (1998)
Ascorbic acid-L (additives) IFU Method No 17a (1995) HPLC
Fruit Juices and Ascorbic-L (additives) AOAC 967.21 Indophenol method
Nectars IFU Method No 17

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Methods of analysis for the proposed draft Codex General Standard for Fruit Juices and Nectars (extract from the report of the TFFJ)
The CCMAS reminded the Task Force that the methods proposed by the Codex commodity committee for endorsement should correspond to provisions in Codex standards. In order to
overcome this problem and recognizing that a single method cannot be used to determine the overall authenticity, composition, and quality and that a combination of methods may be used, the
Task Force added the following wording to Section 3 - Essential Composition and Quality Factors.
Section 3.3 - Authenticity
Authenticity is the maintenance of the products essential physical, chemical, organoleptical, and nutritional characteristics of the fruit(s) from which it comes.
Section 3.4 - Verification of Composition, Quality, and Authenticity
Fruit juices and nectars should be subject to testing for authenticity, composition, and quality where applicable and where required. The analytical methods used should be those found in
Section 8, Methods of Analysis and Sampling.
The Task Force noted that the question of establishing specific values for fruit juices corresponding to each method of analysis was complicated and required a new approach. The Task Force
was of the view that previous fruit juice standards applied to a very small number of juices from specific fruits and that the current General Standard being developed covered a much wider
range of juices, their mixtures and other fruit juice products and that a number of different methods were used internationally, therefore it was not possible to agree on the specific values at this
stage. The Task Force concluded that the approach used by this Task Force should be to develop and only then agree upon specific values for all the varieties of fruit juices and other products
covered by the General Standard on Fruit Juices and Nectars using the proposed methodology (ALINORM 03/39A, paras. 69-71 and 76).

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 Not specified Determination of ash in fruit products Gravimetry
AOAC 940.26 (JAOAC 23, 314 (1940))
EN 1135 (1994) - IFU Method No 9 (1989)
Not specified Determination of Beet sugar in fruit juices Deuterium NMR
AOAC 995.17 - JAOAC 79, 917 (1996)
Determination of Benzoic acid as a marker in orange juice HPLC
AOAC 994.11 - JAOAC 78, 80 (1995)
Carbon dioxide (additives IFU Method No 42 (1976) Titrimetry
and processing aids) (back-titration after precipitation)
Not specified Determination of C13/C12 ratio of ethanol derived from fruit juices Stable isotope mass spectrometry
Method Submitted to AOAC

Not specified Determination of Carbon stable isotope ratio of apple juice Stable isotope mass spectrometry
AOAC 981.09 - JAOAC 64, 85 (1981)

Not specified Determination of Carbon stable isotope ratio of orange juice Stable isotope mass spectrometry
AOAC 982.21 - JAOAC 65, 608 (1982)
[Link] Chem, 29, 803-804 (1981)
Not specified Determination of Carotenoid, Total/individual groups Precipitation/fractionation
EN 12136 (1997) - IFU Method No59 (1991)

Not specified Determination of Centrifugable pulp Centrifugation/% value

EN 12134 - IFU Method No 60 (1991/1998)
Not specified Determination of Chloride (expressed as sodium chloride) Electrochemical titrimetry
EN12133
IFU Method No 37 (1968)
Not specified Determination of Chloride in vegetable juice Titration
AOAC 971.27 (Codex general method)
Fruit Juices and Citric acid (additives) AOAC 986.13 HPLC
Nectars JAOAC 69, 594 (1986)
JAOAC 77, 411 (1994)
Citric acid, enzyme EN 1137 Enzymatic determination
(additives) IFU Method No 22 (1985)
Not specified Determination of Essential oils (Scott) distillation, titration
AOAC 968.20 - IFU 45b
Not specified Determination of Fermentability Microbiological method
IFU Method No 18 (1974)
9
 Not specified Determination of Formol number Potentiometric titration
EN 1133 (1994)
IFU Method No 30 (1984)
Not specified Determination of Free amino acids EN 12742 Chromatography
IFU Method No 57 (1989)
Not specified Determination of Fumaric acid HPLC
IFU Method No 72 (1998)
Glucose and fructose EN 12630 HPLC
(permitted ingredients) IFU Method No 67 (1996)
Not specified Determination of sorbitol
EN 12630
IFU Method No 67 (1996)
Glucose-D and fructose-D EN 1140 Enzymatic determination
(permitted ingredients) IFU Method No 55 (1985)
Not specified Determination of Gluconic acid
IFU Method No 76 (2001)
Not specified Determination of Glycerol
IFU Method No 77 (2001)
Not specified Determination of hesperidin and naringin HPLC
EN 12148 (1996) - IFU Method No 58 (1991)
HFCS & HIS in apple juice JAOAC 84, 486 (2001) CAP GC Method
(permitted ingredients)
Not specified Determination of Hydroxymethylfurfural HPLC
IFU Method No 69 (1996)
Not specified Determination of Isocitric acid-D Enzymatic determination
EN 1139 - IFU Method No 54 (1984)
Fruit Juices and Not specified Determination of Lactic acid- D and L Enzymatic determination
Nectars EN 12631 (1999)
IFU Method No 53 (1983/1996)
Malic acid (additives) AOAC 993.05, JAOAC 69, 594 (1986); JAOAC 77, 411 (1994) Enzymatic determination and HPLC

Not specified Determination of (L-malic/total malic acid ratio in apple juice)

AOAC 993.05, JAOAC 69, 594 (1986)
JAOAC 77, 411 (1994)

Malic acid-D EN 12138 Enzymatic determination

IFU Method No 64 (1995)

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 Malic acid-D in apple juice AOAC 995.06 HPLC
Malic acid-L EN 1138 (1994) Enzymatic
IFU Method No 21 (1985)
Not specified Determination of Naringin and neohesperidin in orange juice HPLC
AOAC 999.05
JAOAC, Vol. 83, No.5 (2000), pp1155-1165
Pectin (additives) IFU Method No 26 (1964/1996) Precipitation/photometry

Not specified Determination of pH-value Potentiometry

EN 1132 (1994)
IFU Method No 11 (1968/1989)
Not specified Determination of Phosphorus/Phosphate Photometric determination
EN 1136 (1994)
IFU Method No 50 (1983)
Preservatives in fruit juices8 IFU Method No 63 (1995) HPLC

Not specified Determination of Proline Photometry

EN 1141 (1994)
IFU Method No 49 (1983)
Quinic, malic & citric acid AOAC 986.13 HPLC
in cranberry juice cocktail JAOAC 69, 594 (1986)
and apple juice (permitted
ingredients and additives)
Not specified Determination of Recoverable oil Distillation and titration Scott method
AOAC 968.20 - IFU Method No 45b
Not specified Determination of Relative density Pycnometry
EN 1131 (1993)
IFU Method No 1 (1989) &
IFU Method No General sheet (1971)
Not specified Determination of Relative density Densitometry
IFU Method No 1A
Not specified Determination of Sodium, potassium, calcium, magnesium Atomic Absorption Spectroscopy
EN 1134 (1994)
IFU Method No 33 (1984)

8
Benzoic acid and its salts; sorbic acid and its salts
11
Soluble solids AOAC 983.17 Indirect by refractometry
EN 12143 (1996)
IFU Method No 8 (1991)
Not specified Determination of Sorbitol-D Enzymatic determination
IFU Method No 62 (1995)
Not specified Determination of Stable carbon isotope ratio
in the pulp of fruit juices
ENV 13070 (1998)
Analytica Chimica Acta 340 (1997)
Not specified Determination of Stable carbon isotope ratio of sugars from fruit juices Stable isotope mass spectrometry
ENV 12140
Analytica Chimica Acta.271 (1993)

Not specified Determination of Stable hydrogen isotope ratio of water from fruit juices Stable isotope mass spectrometry
ENV 12142 (1997)

Not specified Determination of Stable oxygen isotope ratio in fruit juice water Stable isotope mass spectrometry
ENV 12141(1997)

Not specified Determination of Starch

AOAC 925.38
IFU Method No 73
Sucrose (permitted EN 12146 (1996) Enzymatic determination
ingredients) IFU Method No 56 (1985/1998)
Sucrose (permitted EN 12630 HPLC
ingredients) IFU Method No 67 (1996)
Not specified Determination of Sugar -beet derviced syrups Oxygen isotope ratio analysis
in frozen concentrated orange juice 18O Measurements in Water - AOAC
992.09
Not specified Determination of Sulfates Precipitation/Gravimetry
EN 1142 (1994)
IFU Method No 36 (1987)
Suphites (additives and Determination of Sulphur dioxide by modified Powell Titrimetry after distillation
processing aids) EN 13196 not identical with
IFU Method No Method No 7A (2000)
Suphites (additives and Determination of Sulphur dioxide by Optimized Monier Williams AOAC Titrimetry after distillation
processing aids) 990.28

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 Tartaric acid in grape juice EN 12137 (1997) HPLC
(additives) IFU Method No 65 (1995)
Not specified Determination of Titrable acids, total Titrimetry
EN 12147 (1995)
IFU Method No Method No 3, (1968)
Not specified Determination of Total dry matter
EN 12145 (1996)
IFU Method No 61 (1991)
Not specified Determination of Total nitrogen Digestion/titration
EN 12135 (1997)
IFU Method No 28 (1991)
Not specified Determination of Total solids Microwave oven drying
AOAC 985.26
Not specified Determination of Vitamin C Microfluorometry
AOAC 967.22
Not specified Determination of Vitamin C - CEN DNA

Part II. SAMPLING

CODEX COMMITTEE ON FATS AND OILS (ALINORM 03/17, Appendix II)
Standard for Olive Oils and Olive-Pomace Oils
Sections 8.16 and Annex-Section 4.12 Sampling
According to ISO 661:1989 and ISO 5555:2001.

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